Method of purifying silicon utilizing cascading process

• US 8,580,218 B2
• Filed: 06/12/2012
• Issued: 11/12/2013
• Est. Priority Date: 08/21/2009
• Status: Active Grant

• Current Assignee: Highland Materials Incorporated
• Original Assignee: Silicor Materials, Inc.
• Inventors: Turenne, Alain, Nichol, Scott, Smith, Dan
• Primary Examiner(s): Zimmer, Anthony J
• Application Number:
  US13/494,710
• Publication Number:
  US 20120260850A1
• Time in Patent Office: 518 Days
• Field of Search: 423348-350
• US Class Current: 423/348
• CPC Class Codes: C01B 33/037 Purification by zone-melting C30B13/00
• CPC Class Codes: C01P 2006/80 Compositional purity

Abstract

The present invention relates to a method of purifying a material using a metallic solvent. The present invention includes a method of purifying silicon utilizing a cascade process. In a cascade process, as the silicon moves through the purification process, it contacts increasingly pure solvent metal that is moving through the process in an opposite direction.

Claims

1. A method for purifying metallurgical grade (MG) silicon, comprising:

(a) contacting a first silicon with a second mother liquor, to provide a first mixture;

(b) melting the first mixture to a temperature above the liquidus, to provide a first molten mixture;

(c) cooling the first molten mixture to a temperature below the solidus, to form first silicon crystals and a third mother liquor;

(d) separating the first silicon crystals and the third mother liquor;

(e) contacting the first silicon crystals and a first mother liquor, to provide a second mixture;

(f) melting the second mixture to a temperature above the liquidus, to provide a second molten mixture;

(g) cooling the second molten mixture to a temperature below the solidus, to form second silicon crystals and a second mother liquor;

(h) separating the second silicon crystals and the second mother liquor;

(i) contacting the second silicon crystals with a first solvent metal, to provide a third mixture;

(j) melting the third mixture to a temperature above the liquidus, to provide a third molten mixture;

(k) cooling the third molten mixture to a temperature below the solidus, to form third silicon crystals and a first mother liquor; and

(l) separating the third silicon crystals and the first mother liquor;

wherein the mother liquors and the first solvent metal comprise a solvent metal;

wherein the method provides upgraded metallurgical-grade (UMG) silicon; and

further comprising combining the first mother liquor with at least a portion of the second mother liquor prior to contacting the first mother liquor with the first silicon crystals.

2. The method of claim 1, wherein the method provides upgraded metallurgical-grade (UMG) silicon with boron levels less than 0.75 ppmw, aluminum levels less than 1.0 ppmw, phosphorous levels less than 0.8 ppmw and other metallic element levels totaling less than 1 ppmw, wherein the other metallic elements comprise one or more of magnesium, titanium, manganese, iron, cobalt, nickel, copper, zinc, molybdenum, cadmium, tin, tungsten, lead and uranium.

3. The method of claim 1, further comprising combining the second mother liquor with at least a portion of the third mother liquor prior to contacting the second mother liquor with the first silicon.

4. The method of claim 3, wherein the first mother liquor contains more of the solvent metal, compared to the second mother liquor.

5. The method of claim 1, further comprising removing at least a portion of the solvent metal from the third silicon crystals.

6. The method of claim 1, further comprising mechanically removing a powder, the solvent metal, a contaminate, or some combination thereof from the third silicon crystals.

7. The method of claim 1, further comprising melting the third silicon crystals to a temperature above the liquidus.

8. The method of claim 7, further comprising contacting a gas, slag molten silicon or some combination thereof to the molten third silicon crystals.

9. The method of claim 8, further comprising directionally solidifying silicon from the molten third silicon crystals, to form an ingot.

10. The method of claim 9, further comprising removing a portion of the ingot.

11. The method of claim 10, wherein the steps of directionally solidifying and removing at least a portion of the ingot are repeated one or more times.

12. The method of claim 1, wherein steps (a)-(d) are repeated one or more times.

13. The method of claim 1, wherein steps (e)-(h) are repeated one or more times.

14. The method of claim 1, wherein one or more of the mother liquors or the molten mixtures or a combination thereof are cleaned using a ceramic foam filter or gas injection containing chlorine.

15. The method of claim 8, further comprising cleaning the molten silicon with a ceramic foam filter or gas injection containing chlorine.

16. The method of claim 1, wherein the solvent metal comprises aluminum.

17. The method of claim 5, wherein removing comprises dissolving or reacting or a combination thereof with acid, base or other chemical.

18. The method of claim 8, wherein the gas comprises oxygen.

19. A method for purifying metallurgical grade (MG) silicon, comprising:

(a) contacting a first silicon with a second mother liquor, to provide a first mixture;

(b) melting the first mixture to a temperature above the liquidus, to provide a first molten mixture;

(c) cooling the first molten liquid to a temperature below the solidus, to form first silicon crystals and a third mother liquor;

(d) separating the first silicon crystals and the third mother liquor;

(e) contacting the first silicon crystals and a first mother liquor, to provide a second mixture;

(f) melting the second mixture to a temperature above the liquidus, to provide a second molten mixture;

(g) cooling the second molten liquid to a temperature below the solidus, to form second silicon crystals and a second mother liquor;

(h) separating the second silicon crystals and the second mother liquor;

(i) contacting the second silicon crystals with a first solvent metal, to provide a third mixture;

(j) melting the third mixture to a temperature above the liquidus, to provide a third molten mixture;

(k) cooling the third molten liquid to a temperature below the solidus, to form third silicon crystals and a first mother liquor;

(l) separating the third silicon crystals and the first mother liquor;

(m) melting the third silicon crystals, to provide melted third crystals to a temperature above the liquidus;

(n) directionally solidifying the melted third crystals, to provide a solidified silicon; and

(o) removing at least a portion of the solidified silicon;

wherein the mother liquors and the first solvent metal comprise a solvent metal,

wherein the solvent metal comprises aluminum, and

wherein the method provides upgraded metallurgical-grade (UMG) silicon; and

further comprising combining the first mother liquor with at least a portion of the second mother liquor prior to contacting the first mother liquor with the first silicon crystals.

20. The method of claim 19, wherein the method provides upgraded metallurgical-grade (UMG) silicon with boron levels less than 0.75 ppmw, aluminum levels less than 1.0 ppmw, phosphorous levels less than 0.8 ppmw and other metallic element levels totaling less than 1 ppmw, wherein the other metallic elements comprise one or more of magnesium, titanium, manganese, iron, cobalt, nickel, copper, zinc, molybdenum, cadmium, tin, tungsten, lead and uranium.

21. The method of claim 19, further comprising, prior to step (n), contacting the melted third crystals with at least one of a gas or slag molten silicon.

22. The method of claim 19, further comprising repeating step (m) through (o) one or more times.

23. A method for purifying metallurgical grade (MG) silicon, comprising:

(a) contacting a silicon A with a third mother liquor, to provide a mixture A;

(b) melting the mixture A to a temperature above the liquidus, to provide a molten mixture A;

(c) cooling the molten liquid A to a temperature below the solidus, to form a first silicon and a fourth mother liquor;

(d) separating the first silicon and the fourth mother liquor;

(e) contacting the first silicon with a second mother liquor, to provide a first mixture;

(f) melting the first mixture to a temperature above the liquidus, to provide a first molten mixture;

(g) cooling the first molten liquid to a temperature below the solidus, to form first silicon crystals and a third mother liquor;

(h) separating the first silicon crystals and the third mother liquor;

(i) contacting the first silicon crystals and a first mother liquor, to provide a second mixture;

(j) melting the second mixture to a temperature above the liquidus, to provide a second molten mixture;

(k) cooling the second molten liquid to a temperature below the solidus, to form second silicon crystals and a second mother liquor;

(l) separating the second silicon crystals and the second mother liquor;

(m) contacting the second silicon crystals with a first solvent metal, to provide a third mixture;

(n) melting the third mixture to a temperature above the liquidus, to provide a third molten mixture;

(o) cooling the third molten liquid to a temperature below the solidus, to form third silicon crystals and a first mother liquor;

(p) separating the third silicon crystals and the first mother liquor;

(q) melting the third silicon crystals to a temperature above the liquidus, to provide melted third crystals;

(r) directionally solidifying the melted third crystals, to provide a solidified silicon; and

(s) removing at least a portion of the solidified silicon

wherein the mother liquors and the first solvent metal comprise a solvent metal,

wherein the solvent metal comprises aluminum,

wherein steps (a)-(d) are repeated zero times, once, or twice,

herein steps (e)-(h) are repeated zero times, once, or twice,

herein steps (i)-(l) are repeated zero times, once, or twice,

wherein steps (m)-(p) are repeated zero times, once, or twice,

wherein steps (q)-(s) are repeated zero times, once, or twice,

wherein the method provides upgraded metallurgical-grade (UMG) silicon, and

wherein other metallic elements comprise one or more of magnesium, titanium, manganese, iron, cobalt, nickel, copper, zinc, molybdenum, cadmium, tin, tungsten, lead and uranium; and

further comprising combining the second mother liquor with at least a portion of the third mother liquor prior to contacting the second mother liquor with the first silicon.

24. The method of claim 23, wherein the method provides upgraded metallurgical-grade (UMG) silicon with boron levels less than 0.75 ppmw, aluminum levels less than 1.0 ppmw, phosphorous levels less than 0.8 ppmw and other metallic element levels totaling less than 1 ppmw.